CN106336207A - 一种异形结构石英陶瓷制品的制备方法 - Google Patents

一种异形结构石英陶瓷制品的制备方法 Download PDF

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CN106336207A
CN106336207A CN201610726737.0A CN201610726737A CN106336207A CN 106336207 A CN106336207 A CN 106336207A CN 201610726737 A CN201610726737 A CN 201610726737A CN 106336207 A CN106336207 A CN 106336207A
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麦浩
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Bright Cities And Towns Gaoming District Foshan City New Forms Of Energy New Material Industry Innovation Centers
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Abstract

本发明公开了一种异形结构石英陶瓷制品的制备方法，包括步骤A、将高纯熔融石英粉料进行混合；将上述高纯熔融石英粉料加入乳酸和碳酸氢三钠，搅拌均匀得到混合粉料；B、称取占步骤A中石英粉料质量12‑18%的粘结剂，在水浴中加热融化，然后将步骤A中制备的混合粉料倒入粘结剂中，搅拌均匀，得到浆料；C、将步骤B中制得的浆料注入至模具中，利用模具的冷却系统对浆料进行降温使其冷却凝固，取出成型坯体；D、将步骤C中的成型坯体进行加热，直至成型坯体中的氧化聚乙烯蜡和凡士林全部蒸发或者流出，再将炉温升至1100‑1300℃进行烧制，保温5‑6h，随炉冷却，即得到所需石英陶瓷制品。

Description

一种异形结构石英陶瓷制品的制备方法
技术领域
本发明属于石英陶瓷制备领域，具体涉及一种复杂结构石英陶瓷制品的制备方法。
背景技术
石英陶瓷是指以石英玻璃或者熔融石英为原料，经破碎、成型、烧成扥公益系列陶瓷制作工艺制备的制品，又称为熔融石英陶瓷、石英玻璃陶瓷、石英玻璃烧结制品等。石英陶瓷由于具有热膨胀系数好、热震稳定性好、耐化学侵蚀性号等优点，得到了广泛的应用。但是，由于石英陶瓷粘度大，挥发性也随着温度的升高而增加，故而难以用通常生产硅酸盐玻璃制品的工艺来生产大型的形状复杂的石英陶瓷制品。
目前的技术中大都采用石膏模型泥浆浇注成型的方法来生产石英陶瓷类制品，该方法有以下缺点：1）利用石膏模型，石英陶瓷制品的外观形状容易保证，但是内部结构无法保证，一旦模型过于复杂或者不均匀，陶瓷制品内部易出现气泡、团聚等现象；2）无法制备成型厚度较大和形状复杂的石英陶瓷制品；3）无法利用粒度较大的原料。在许多需要制备异形结构（如厚薄不均匀的制件、结构复杂的制件等）石英陶瓷制品的应用中，使用泥浆浇注的工艺方法无法满足需求。
发明内容
考虑到现有技术中制备石英陶瓷制品工艺中存在的问题，本发明中并不采用现有技术中水作为石英粉料料浆中的液相，而是将石英粉料在添加了助剂之后与融化的粘结剂进行混合，增强了其流动性和粉料之间的连接力，良好的解决了形状和内部结构较为复杂的石英陶瓷制品的成型问题。
本发明所要解决的技术问题通过以下步骤予以实现：
本发明提供的一种异形结构石英陶瓷制品的制备方法，包括如下步骤：
A、将高纯熔融石英粉料进行混合，其中熔融石英粉料的粒度分布及所占质量分数为：1-5μm，5-10%；5-18μm，5-10%；18-30μm，10-20%；30-40μm，35-40%；40-60μm，18-25%；60-100μm，8-15%；将上述高纯熔融石英粉料加入占石英粉料质量为0.5-0.6%的乳酸和0.1-0.2%碳酸氢三钠，搅拌均匀得到混合粉料；
B、称取占步骤A中石英粉料质量12-18%的粘结剂，在水浴中加热融化，然后将步骤A中制备的混合粉料倒入粘结剂中，搅拌均匀，得到浆料；
所述粘结剂的成分及质量百分数为：氧化聚乙烯蜡70-86wt%、凡士林5-15wt%、蜂蜡5-10wt%、松香2-5wt%；
C、将步骤B中制得的浆料注入至模具中，利用模具的冷却系统对浆料进行降温使其冷却凝固，取出成型坯体；
D、将步骤C中的成型坯体进行加热，直至成型坯体中的氧化聚乙烯蜡和凡士林全部蒸发或者流出，再将炉温升至1100-1300℃进行烧制，保温5-6h，随炉冷却，即得到所需石英陶瓷制品。
本发明中严格控制熔融石英粉料的粒度范围和所占的质量百分比，并添加适量乳酸和碳酸氢三钠作为表面活性剂，主要目的是使熔融石英粉料能够均匀分散在粘结剂中，并且有助于增强浆料的流动性。粘结剂采用氧化聚乙烯蜡、凡士林、蜂蜡和松香的混合物，其中质量稳定流动性好的氧化聚乙烯蜡作为粘结剂的主体成分，再进一步优选，氧化聚乙烯蜡分子量为1800-2000。氧化聚乙烯蜡分子链带有一定量的羰基和羟基，所以在由有机物构成的极性体系中其润湿性和分散性尤启佳，能够非常有效的将熔融石英粉料结合在一起，同时流动性好。
进一步优选原料，步骤A中的高纯熔融石英粉料纯度大于99.99wt%。
进一步地，步骤A中的高纯熔融石英粉料中还加入占其质量百分比为0.5-1.0%的Si3N4粉体、Al2O3粉体、MgO粉体中的一种。所述添加的粉体粒径为10-40μm。所述添加的粉体粒径为20-60μm。该步骤中添加的矿物粉体一方面可作为烧结助剂存在，另一方面适量添加上述粉体可有效抑制在烧结过程中的析晶过程，减少石英陶瓷制品内部缺陷。
进一步优选地，步骤B中融化粘结剂的水浴温度为80-90℃。
进一步优选地，步骤C中加热成型坯体至聚乙烯蜡和凡士林全部蒸发或者流出的环境温度为120-140℃。再进一步优选范围，步骤C中加热成型坯体至聚乙烯蜡和凡士林全部蒸发或者流出的环境温度为135-140℃。
进一步地，步骤D中烧制成型步骤具体为：以4-6℃/min由室温升至600℃，保温20min后，再以7-10℃/min升至1050-1250℃，保温后随炉冷却。
熔融石英陶瓷受到方石英析晶的影响，烧制成型的温度不宜超过1300℃。本发明中先升温至600℃，然后通过快速升温至所需烧结温度，可在最大程度上控制烧制成型的收缩率。添加适量的烧结助剂有助于进一步提高注凝成型制品的烧结程度和致密程度。
本发明具有如下有益效果：
1、本发明中的石英陶瓷制品的制备方法不采用现有技术中的石膏模型泥浆浇注成型的方法，而是采用将石英粉料在添加了助剂之后与融化的粘结剂进行混合，然后通过加热除去粘结剂，最后进行烧制的工艺过程，利用本发明中的方法增强了粉体浆料的流动性和粉料颗粒之间的连接力，良好的解决了形状和内部结构较为复杂的石英陶瓷制品的成型问题。
2、通过本发明中提供的方法可制备出设计较为复杂结构的异形结构石英陶瓷制品，而且制备得到的石英陶瓷制品外观良好、内部缺陷少。
具体实施方式
下面通过实施例对本发明的内容进行进一步的描述。
实施例1
步骤1：粉料混合
选择的高纯熔融石英粉料原料纯度大于99.99wt%。
将所选择的熔融石英粉料进行混合，其中熔融石英粉料的粒度分布及所占质量分数为：1-5μm，5%；5-18μm，10%；18-30μm， 20%；30-40μm，35%；40-60μm，20%；60-100μm，10%；将上述高纯熔融石英粉料加入占石英粉料质量为0.55%的乳酸和0.15%碳酸氢三钠，搅拌均匀得到混合粉料。
相比起普通熔融石英陶瓷制品的原材料选择，本实施例中选择的熔融石英原料粉体整体粒度偏小，主要是考虑到粘结剂与粉体材料的相容性和后续烧制步骤的效率问题，选用整体粒度偏小的原料粉体一方面可提升粘结剂与粉体混合后的均匀程度，另一方面可有效提升烧成步骤的效率。
步骤2：制备浆料
将85wt%氧化聚乙烯蜡、9wt%凡士林、4wt%蜂蜡、2wt%松香进行混合制成粘结剂，在90℃水浴中加热融化，然后将步骤1中的混合粉料倒入粘结剂中，搅拌均匀，得到浆料，其中粘结剂质量为步骤1中石英粉料质量的14%。
粘结剂中使用的氧化聚乙烯蜡分子量为1800-2000，氧化聚乙烯蜡分子量一旦超过2000则流动性会达不到要求。该步骤中所选择的凡士林也同样如此进行选择，可尽量选择市售产品中分子量较小的产品，流动性更好。
步骤3：制坯、烧成
将步骤2中制得的浆料注入至模具中，利用模具的冷却系统对浆料进行降温使其冷却凝固，取出成型坯体。
将成型坯体在140℃条件下持续加热，直至成型坯体中的聚乙烯蜡和凡士林全部蒸发或者流出，再将炉温升至1150℃进行烧制，保温6h，随炉冷却，即得到所需石英陶瓷制品。烧制成型步骤具体为：以5℃/min由室温升至600℃，保温20min后，再以10℃/min升至1150℃，保温后随炉冷却。
实施例2
本实施例中工艺条件及原料与实施例1保持一致，不同点在于：步骤1中高纯熔融石英粉料中还添加有占其质量百分比为0.6%的Si3N4粉体。粉体粒径为10μm。
实施例3
本实施例中工艺条件及原料与实施例1保持一致，不同点在于：步骤1中高纯熔融石英粉料中还添加有占其质量百分比为1%的Al2O3粉体。粉体粒径为15μm。
实施例4
本实施例中工艺条件及原料与实施例1保持一致，不同点在于：步骤1中高纯熔融石英粉料中还添加有占其质量百分比为1%的MgO粉体。粉体粒径为15μm。
实施例1-4中烧制出的石英陶瓷制品表面光洁平整，外观无可见缺陷，通过机械切割方式观察内部烧制的情况，也未观察到明显缺陷。相比起普通泥浆浇注制备的石英陶瓷制品，实施例中的陶瓷制品内部几乎无缺陷（无气泡无凸起），适用于制备复杂结构的石英陶瓷制品。
最后需要说明的是，以上实施例仅用以说明本发明实施例的技术方案而非对其进行限制，尽管参照较佳实施例对本发明实施例进行了详细的说明，本领域的普通技术人员应当理解依然可以对本发明实施例的技术方案进行修改或者等同替换，而这些修改或者等同替换亦不能使修改后的技术方案脱离本发明实施例技术方案的范围。

Claims (9)

1.一种异形结构石英陶瓷制品的制备方法，其特征在于包括如下步骤：
A、将高纯熔融石英粉料进行混合，其中熔融石英粉料的粒度分布及所占质量分数为：1-5μm，5-10%；5-18μm，5-10%；18-30μm，10-20%；30-40μm，35-40%；40-60μm，18-25%；60-100μm，8-15%；将上述高纯熔融石英粉料加入占石英粉料质量为0.5-0.6%的乳酸和0.1-0.2%碳酸氢三钠，搅拌均匀得到混合粉料；
B、称取占步骤A中石英粉料质量12-18%的粘结剂，在水浴中加热融化，然后将步骤A中制备的混合粉料倒入粘结剂中，搅拌均匀，得到浆料；
所述粘结剂的成分及质量百分数为：氧化聚乙烯蜡70-86wt%、凡士林5-15wt%、蜂蜡5-10wt%、松香2-5wt%；
C、将步骤B中制得的浆料注入至模具中，利用模具的冷却系统对浆料进行降温使其冷却凝固，取出成型坯体；
D、将步骤C中的成型坯体进行加热，直至成型坯体中的氧化聚乙烯蜡和凡士林全部蒸发或者流出，再将炉温升至1100-1300℃进行烧制，保温5-6h，随炉冷却，即得到所需石英陶瓷制品。
2.如权利要求1所述的制备方法，其特征在于：步骤A中的高纯熔融石英粉料纯度大于99.99wt%。
3.如权利要求1所述的制备方法，其特征在于：步骤A中的高纯熔融石英粉料中还加入占其质量百分比为0.5-1.0%的Si3N4粉体、Al2O3粉体、MgO粉体中的一种。
4.如权利要求3所述的制备方法，其特征在于：所述添加的粉体粒径为10-40μm。
5.如权利要求1所述的制备方法，其特征在于：步骤B中氧化聚乙烯蜡分子量为1800-2000。
6.如权利要求1所述的制备方法，其特征在于：步骤B中融化粘结剂的水浴温度为80-90℃。
7.如权利要求1所述的制备方法，其特征在于：步骤C中加热成型坯体至聚乙烯蜡和凡士林全部蒸发或者流出的环境温度为120-140℃。
8.如权利要求7所述的制备方法，其特征在于：步骤C中加热成型坯体至聚乙烯蜡和凡士林全部蒸发或者流出的环境温度为135-140℃。
9.如权利要求1所述的制备方法，其特征在于：步骤D中烧制成型步骤具体为：以4-6℃/min由室温升至600℃，保温20min后，再以7-10℃/min升至1050-1250℃，保温后随炉冷却。
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